羟基磷灰石改性膨润土对铀的吸附效果及其机制

张益硕; 周仲魁; 李龙祥; 郭亚丹; 孙占学

羟基磷灰石改性膨润土对铀的吸附效果及其机制

张益硕^{1, 2},
周仲魁^{1, 2, ,},
李龙祥^{1, 2},
郭亚丹^{1, 2},
孙占学^{1, 2}

1.
东华理工大学　核资源与环境国家重点实验室, 南昌 330013
2.
东华理工大学　水资源与环境工程学院, 南昌 330013

基金项目: 国家自然科学基金 (41662024)；江西省重点研发计划重点项目(20212BBG71011)

详细信息

通讯作者:
周仲魁，博士，教授，硕士生导师，研究方向为铀矿山环境治理与修复　E-mail: zhkzhou80@163.com

中图分类号: X703.1
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- 文章访问数: 109
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- 被引次数: 0
出版历程
- 收稿日期: 2023-02-01
- 修回日期: 2023-02-26
- 录用日期: 2023-03-03
- 网络出版日期: 2023-03-18

Study on adsorption effect and mechanism of uranium by hydroxyapatite modified bentonite

Yishuo ZHANG^{1, 2},
Zhongkui ZHOU^{1, 2
, ,},
Longxiang LI^{1, 2},
Yadan GUO^{1, 2},
Zhanxue SUN^{1, 2}

1.
State Key Laboratory of Nuclear Resources and Environment, East China University of Technology, Nanchang 330013, China
2.
School of Water Resources and Environmental Engineering, East China University of Technology, Nanchang 330013, China

Funds: National Natural Science Foundation of China(41662024)；Key Projects of Jiangxi Province Key R&D Programme (20212BBG71011)

摘要

摘要: 膨润土(BTN)的团聚性(图1)及缺少吸附官能团严重制约其对含铀废水的去除性能，需对其进行改性使其成为复合材料以提高膨润土的吸附性能。1膨润土TEM图TEM diagram of bentonite本文以膨润土、磷酸氢二钠、硝酸钙为原料，采用简单易行的一步水热法成功制备出羟基磷灰石改性膨润土复合材料(HAP/BTN)，即克服了膨润土的团聚性又使吸附材料的制备简单化，且由于HAP/BTN的组成为天然膨润土和羟基磷灰石，因此，其对环境产生的二次污染较小，提升了环境吸附材料的工业应用潜力。本工作采用较成熟的单因素试验和正交试验考察了HAP/BTN吸附铀的性能，得出其对铀的去除率可达98%，吸附等温线拟合得出其吸附量为186.45 mg/g，最后通过表征及Zeta电位分析得出其吸附机制如图2所示。2HAP/BTN吸附铀机制Mechanism of uranium adsorption by HAP/BTN
- 膨润土 /
- 羟基磷灰石 /
- 铀废水 /
- 吸附 /
- U(VI)
Abstract: With the development and efficient utilization of nuclear energy in China, uranium has become one of the common pollutants in surface water, groundwater and soil. The removal of U(VI) from uranium-containing wastewater has become an urgent environmental problem to be solved. Hydroxyapatite modified bentonite composite hydroxyapatite modified bentonite (HAP/BTN) was successfully prepared by a simple one-step hydrothermal method using bentonite, disodium hydrogen phosphate and calcium nitrate as raw materials. The adsorption performance of HAP/BTN on uranium in wastewater was investigated. The effects of pH, rotation speed, temperature, dosage and time on the adsorption performance were discussed by orthogonal test. The results showed that under the conditions of pH=6.0, rotation speed=100 r·min⁻¹, room temperature (298.15 K), HAP/BTN dosage of 1 g·L⁻¹ and t=30 min, the removal rate of 10 mg·L⁻¹ uranium-containing wastewater could reach 98%, and the maximum adsorption capacity was 186.45 mg·g⁻¹. The adsorption process was more in line with the Langmuir model and pseudo-second-order kinetics. Thermodynamic parameters show that the adsorption of uranium on HAP/BTN was a spontaneous endothermic process, combined with XPS and XRD results, confirmed that the adsorption of uranium by HAP/BTN was mainly attributed to complexation reaction, chemical adsorption, electrostatic and ion exchange.
- Bentonite /
- hydroxyapatite /
- uranium wastewater /
- adsorption /
- U(VI)

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图 1 BTN的TEM图像(a)、羟基磷灰石改性膨润土复合材料(HAP/BTN)的TEM图像(b)

Figure 1. TEM images of BTN (a), TEM images of hydroxyapatite modified bentonite (HAP/BTN) (b)

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图 2 BTN的SEM图像(a)、HAP/BTN的SEM图像(b)

Figure 2. SEM images of BTN (a), SEM images of HAP/BTN (b)

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图 3 HAP/BTN的红外光谱图

Figure 3. Infrared spectra of HAP/BTN

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图 4 HAP/BTN和BTN两种吸附材料对铀的吸附性能比较

Figure 4. Comparison of adsorption properties of HAP/BTN and BTN for uranium

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图 5 pH值对HAP/BTN吸附铀的影响(a)、铀在不同pH下的物种形态(C₀=10 mg·L⁻¹，PCO₂=0.00039 atm)(b)

Figure 5. Effect of pH on uranium adsorption by HAP/BTN (a), Species morphology of uranium at different pH (C₀=10 mg·L⁻¹, PCO₂=0.00039 atm) (b)

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图 6 振荡转速对HAP/BTN吸附铀的影响

Figure 6. Effect of shaking speed on the adsorption of uranium by HAP/BTN

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图 7 投加量对HAP/BTN吸附铀的影响

Figure 7. Effect of dosage on adsorption of uranium by HAP/BTN

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图 8 吸附时间对HAP/BTN吸附铀的影响

Figure 8. Effect of adsorption time on the adsorption of uranium by HAP/BTN

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图 9 水溶液温度对HAP/BTN吸附铀的影响

Figure 9. The effect of aqueous solution temperature on the adsorption of uranium by HAP/BTN

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图 10 铀溶液体积对HAP/BTN吸附铀的影响

Figure 10. The effect of uranium solution volume on the adsorption of uranium by HAP/BTN

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图 11 铀废水初始浓度对HAP/BTN吸附铀的影响

Figure 11. Effect of initial concentration on uranium adsorption by HAP/BTN

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图 12 材料粒径对HAP/BTN吸附铀的影响(a)、材料煅烧温度对HAP/BTN吸附铀的影响(b)

Figure 12. The effect of particle size on the adsorption of HAP/BTN(a), Effect of calcination temperature on the adsorption of uranium by HAP/BTN(b)

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图 13 HAP/BTN吸附铀的Langmuir和Freundlich拟合曲线(a)、不同铀浓度下HAP/BTN Langmuir等温线吸附模型分离因子(b)

Figure 13. Langmuir and Freundlich fitting curves of uranium adsorption by HAP/BTN (a), Separation factor of HAP/BTN Langmuir isotherm adsorption model at different uranium concentrations(b)

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图 14 HAP/BTN吸附铀的动力学研究：准一级动力学(a)、准二级动力学(b)、Elovich动力学(c)、Morrist颗粒内扩散模型(d)

Figure 14. Kinetic study of uranium adsorption on HAP/BTN： Quasi-first-order kinetics(a), Quasi-second-order kinetics(b), Elovich kinetics(c), Morrist intraparticle diffusion model(d)

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图 15 HAP/BTN对铀(VI)的吸附热力学拟合

Figure 15. Adsorption thermodynamics of uranium (VI) on HAP/BNT

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图 16 HAP/BTN循环试验(a)、BTN或HAP/BTN吸附铀前/吸附后的Zeta电位值(b)、吸附时间对HAP/BTN吸附铀稳定性的影响(c)、不同水样稀释对HAP/BTN吸附铀的影响(pH=6.0，R=100 r•min^-1，T=298.15 K，m=1 g•L^-1，V=50 mL，t=30 min)(d)

Figure 16. HAP/BTN cycle test(a), Zeta potential values of BTN or HAP/BTN before and after adsorption(b), The effect of time on the stability of HAP/BTN(c), Effect of different water samples on H (pH=6.0，R=100 r•min^-1，T=298.15 K，m=1 g•L^-1，V=50 mL，t=30 min) (d)

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图 17 离子强度对HAP/BTN吸附铀的影响(a)、阳离子对HAP/BTN吸附铀的影响(b)、阴离子对HAP/BTN吸附铀的影响(c)

Figure 17. Effect of ionic strength on uranium adsorption by HAP/BTN(a), effect of cations on uranium adsorption by HAP/BTN(b), effect of anions on uranium adsorption by HAP/BTN(c)

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图 18 HAP/BTN吸附铀前后的XPS分析(a, c~e)、铀的精细谱(b)、不同材料的XRD分析(f)、HAP/BTN吸附铀的机制(g)

Figure 18. XPS analysis before and after adsorption of uranium (a,c~e), Fine spectrum of uranium(b), XRD analysis before and after uranium adsorption(f), Adsorption mechanism of HAP/BNT(g)

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图 19 HAP的TEM形貌

Figure 19. TEM morphology of HAP

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表 1 白色块状物质EDS分析

Table 1. EDS analysis of white block material

Element	Mass fraction/%
O	39.07
P	22.65
Ca	38.28

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表 2 HAP/BTN吸附铀的正交试验因素及水平设计

Table 2. Orthogonal test factors and level design of HAP/BTN adsorption of uranium

Factor	A	B	C	D	E
1	2	0	298.15	0.01	1
2	6	60	308.15	0.02	10
3	11	100	318.15	0.05	30
Notes: A—pH of aqueous solution；B—revolution speed/(r·min⁻¹)；C—temperature/K；D—addition amount/g；E—adsorption time/min

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表 3 HAP/BTN吸附铀的正交试验设计方案和结果

Table 3. Orthogonal experimental design and results of HAP / BTN adsorption of uranium

Factor	A	B	C	D	E	S/%
1	2	0	298.15	0.01	1	18.55
2	2	60	308.15	0.02	10	22.32
3	2	100	318.15	0.05	30	24.26
4	6	0	298.15	0.02	10	46.30
5	6	60	308.15	0.05	30	92.05
6	6	100	318.15	0.01	1	71.51
7	11	0	308.15	0.01	30	50.05
8	11	60	318.15	0.02	1	40.76
9	11	100	298.15	0.05	10	70.63
10	2	0	318.15	0.05	10	23.56
11	2	60	298.15	0.01	30	26.78
12	2	100	308.15	0.02	1	20.13
13	6	0	308.15	0.05	1	44.25
14	6	60	318.15	0.01	10	86.12
15	6	100	298.15	0.02	30	99.48
16	11	0	318.15	0.02	30	53.26
17	11	60	298.15	0.05	1	42.14
18	11	100	308.15	0.01	10	74.42
K₁	135.6	235.97	303.88	327.43	237.34
K₂	439.71	310.17	303.22	282.25	323.35
K₃	331.26	360.43	299.47	296.89	345.88
k₁	45.20	78.66	101.29	109.14	79.11
k₂	146.57	103.39	101.07	94.08	107.78
k₃	110.42	120.14	99.823	98.96	115.29
R	101.37	41.48	1.47	15.06	36.18
主次顺序	A>B>E>D>C
Notes: A—pH of aqueous solution；B—revolution speed/(r·min^-1)；C—temperature/K；D—addition amount/g；E—adsorption time/min；K_i—The i (i=1,2,3) level of the factor is the test index.；k_i—the average value of Ki；R-range; S—Adsorption rate

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表 4 HAP/BTN吸附铀的吸附等温线参数

Table 4. Adsorption isotherm parameters of HAP/BTN adsorbing uranium

T	Langmuir			Freundlich
T	q_m/ (mg·g⁻¹)	K_c/ (L·mg⁻¹)	R²	n⁻¹	K_f (mg·g⁻¹)/(mg·L⁻¹)^1/n)	R²
273.15 K	186.45	0.04215	0.99992	0.57112	14.29826	0.91888
Notes: q_m is the saturated adsorption capacity of monolayer adsorption；K_c is a constant related to adsorption energy；K_f is a constant related to the adsorption capacity；n⁻¹ is a measure of the adsorption strength; R²—Correlation coefficient

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表 5 HAP/BTN吸附铀的动力学模型参数

Table 5. HAP/BTN kinetic fitting data

Model types	Equation	q_e/ (mg·g⁻¹)	R²
Pseudo first-order model	ln(q_e−q_t)=−0.10035t+1.26104	3.53	0.911
Pseudo second-order model	t/q=0.09797t+0.14599	9.98	0.997
Elovich model	q_t=0.87196 lnt+6.80159	—	0.981
Morrist intraparticle diffusion model	q_t=0.67023t^1/2+6.52163	—	0.930
	q_t=0.62663t^1/2+6.50141	—	0.961
	q_t=0.299508t^1/2+7.78542	—	0.956
Notes: q_e, q_t—Adsorption amount at time t and adsorption equilibrium, respectively；t—adsorption time；

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表 6 HAP/BTN对铀(VI)的吸附热力学具体参数

Table 6. Thermodynamic parameters of uranium (VI) adsorption on HAP/BTN

T/K	ΔH^θ/ (KJ·mol⁻¹)	ΔS^θ/ (J·mol⁻¹·K⁻¹)	ΔG^θ/ (KJ·mol⁻¹)
298.15	45.27	157.58	−1.71
308.15			−3.29
318.15			−4.86
328.15			−6.44
338.15			−8.01
348.15			−9.59
358.15			−11.16
368.15			−12.76
Notes：ΔH^θ—The heat of the adsorption；ΔS^θ—Standard entropy change；ΔG^θ—Gibbs free energy of adsorption

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